CN102120665B - Method for purifying pentachlorophenol in water through photocatalysis - Google Patents
Method for purifying pentachlorophenol in water through photocatalysis Download PDFInfo
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- CN102120665B CN102120665B CN201110020264A CN201110020264A CN102120665B CN 102120665 B CN102120665 B CN 102120665B CN 201110020264 A CN201110020264 A CN 201110020264A CN 201110020264 A CN201110020264 A CN 201110020264A CN 102120665 B CN102120665 B CN 102120665B
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- pentachlorophenol
- bismuth silicate
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Abstract
The invention relates to a method for purifying pentachlorophenol (PCP) in water through photocatalysis, which comprises the following processes of: mixing and stirring a bismuth silicate photocatalyst and pentachlorophenol sewage to be treated, performing ultrasonic dispersion, adsorbing and balancing, irradiating by using a xenon lamp and the like; and pentachlorophenol photocatalytic degradation reaction results prove that the pentachlorophenol in the water can be efficiently purified through the method. The invention can overcome the defects of high energy consumption, complex operation, violent reaction conditions, poor purification capacity and the like in the conventional purification method, provides a method having the advantages of short flow, simple equipment and good efficiency of purifying the pentachlorophenol, and has wide industrial application prospect.
Description
Technical field
The present invention relates to a kind of purify waste water method of middle Woodtreat A (PCP) of bismuth silicate photocatalyst of utilizing, belong to the surround lighting catalysis technical field.
Background technology
Woodtreat A (PCP) once was widely used as wood preservative, rust-preventive agent, sterilizing agent, sterilant, sterilant and weedicide; Have stench and high toxicity; Be a kind ofly extensively to be present in water body and to have " three cause " (carcinogenic, teratogenesis, mutagenesis) effect and genotoxic organic difficult degradation pollutent; Be difficult for being decomposed and easily through the food chain enrichment in vivo; Thereby natural, ecological and human health are caused serious threat, listed in the list of priority pollutants by EPA.Simultaneously, PCP can also be converted into stronger many chloros dibenzo Dioxins (PCDDs) of toxicity and polychlorinated dibenzo (PCDFs) in physical environment, and it is crucial therefore seeking economy and eco-friendly PCP purification techniques.
Biological process is a kind of effective ways of PCP in purifying waste water, have cost low with easy-operating advantage, but shortcoming such as this method exists long processing period, and big and high density PCP processing efficiency is low to the effect of mikrobe toxicity.Physico-chemical process mainly comprises absorption method, Coagulation Method, extraction process and membrane processing method etc.This method only is PCP from a kind of medium to the process that another kind of medium shifts, and can produce new pollution usually, therefore needs subsequent processes just can reach the purpose of thorough removing PCP.The Sonochemical degradation method exists capacity usage ratio low, and treatment capacity is little, problems such as process cost height.Wet oxidation process needs high-tension apparatus, and apparatus cost is expensive, and catalyst attrition is big, and uneconomical to lower concentration PCP wastewater treatment.There are shortcomings such as current efficiency is low, power consumption is high and lack electrode life in the electrochemical degradation method owing to receive the restriction of electrode materials, therefore is difficult to realize industriallization.
The photocatalytic degradation technology is the novel method of Persistent organic pollutants in a kind of purifying water body that grows up the seventies; Have that energy consumption is low, easy to operate, reaction conditions is gentle, oxidation capacity is strong, with advantage such as environmental compatible, utilization should technology purifies organic wastewater with difficult degradation thereby become the domestic and international research focus.Photocatalyst can produce electron-hole pair under illumination condition, valence band hole (h
+ Vb) have very strong oxidation capacity, can efficiently remove organism in the water; Be adsorbed on the O of catalyst surface simultaneously
2And H
2O can produce various living radicals with the conduction band electron reaction, like hydroxyl radical free radical (OH), ultra-oxygen anion free radical (O
2 -) etc., redox reaction can take place with PCP in these living radicals, and being translated into the low material of toxicity is carbonic acid gas and water with its mineralising perhaps, thereby effectively degrades PCP, has wide prospect in industrial application.
Bi silicate crystals is the non-ferroelectric cube semiconductor of a kind of broad-band gap, high resistivity, has unique photoelectricity, photoconduction, light and sells off and the acousto-optic performance.In recent years, as a kind of important photovaltaic material, bi silicate crystals has caused the great attention of Materials science and photocatalysis field.The patent No. is ZL 200710166218.4, and name is called a kind of preparation method of bismuth silicate powder photocatalyst, and publication number is the preparation method that the patent of CN101157026A has been introduced bismuth silicate in detail.Document " C.H.He, M.Y.Gu.Preparation, characterization and photocatalytic properties of Bi
12SiO
20Powders ScriptaMaterialia 2006 (55): 481-484 " adopt chemical solution decomposition method (CSD) preparation bismuth silicate powder; and investigate its performance Congo red to photocatalytic degradation, the result show illumination after one hour bismuth silicate to Congo red decolorizing efficiency up to 92.1%.
Problem to be solved by this invention is efficiently to remove PCP pollutent in the water, overcomes the existing deficiency that purifies the chlorophenol pollutant technology, and a kind of treatment process of chlorophenols sewage efficient, energy-conservation, simple to operate is provided.
Summary of the invention
The objective of the invention is to solve the pollution problem of PCP in the Industrial processes; Providing a kind of is the method for PCP during photocatalyst is purified waste water with the bismuth silicate; Can overcome existing purifying method energy consumption height, complicated operation, reaction conditions acutely and the shortcoming of detergent power difference, have good economy and environmental benefit.
Utilize bismuth silicate for photocatalyst purify waste water in the method for PCP comprise the steps:
A) the certain density PCP solution of preparation;
B) in PCP solution, add the bismuth silicate photocatalyst;
C) under the dark condition ultrasonic 10 minutes, make the bismuth silicate photocatalyst be dispersed in PCP solution;
D) with c) mixing solutions of step stirs to reach the adsorption equilibrium of PCP at the dark condition lower magnetic force;
E) adopt xenon lamp to shine, the temperature of reaction solution keeps constant temperature through water-bath simultaneously;
F) timing sampling, sample thief supernatant after the spinning, the concentration change of analysis PCP;
G) suction filtration reaction solution, the Separation and Recovery photocatalyst.
The treatment process of PCP sewage of the present invention wherein, is 2～10 mg/litre at the starting point concentration of PCP described in the step a);
The treatment process of PCP sewage of the present invention wherein, is 300～800 nanometers in the xenon lamp wavelength region described in the step e), and power is 500 watts;
Among the present invention, the photocatalysis apparatus that is adopted is made up of direct supply, barretter and xenon lamp, and miscellaneous part comprises quartz reactor, water-bath and magnetic stirring apparatus etc., and used unit all can obtain from relevant device supplier, also can design voluntarily and build.
Analytical procedure to PCP in the water provided by the invention is following:
Adopt performance liquid chromatography (HPLC Waters 1525) to analyze; Moving phase is the mixed solution of the methyl alcohol and the amine acetate aqueous solution (containing 0.02 mol amine acetate); Volume ratio is 85: 15; Flow velocity 1.0 ml/min, it is 312 nanometers that UV-detector is measured wavelength, specimen is removed impurity in order to avoid stop up pillar through 0.45 micron filter membrane.Degradation rate (%)=(initial p CP concentration-residue PCP concentration)/initial p CP concentration * 100%.
The invention has the advantages that:
1. adopt luminous energy to remove PCP in the water, efficiently utilize clean energy;
2. can efficiently remove the pollution of difficult degradation PCP in the water;
3. this method flow is short, equipment is simple, easy to operate, purification rate is high, the photocatalyst easy recovery is utilized, and has good economic benefit and environmental benefit.
This method is that the 250 mg/litre PCP sewage that to handle 200 milliliters of starting point concentrations be 2 mg/litre is after 2 hours at the photocatalyst consumption; Almost can't detect on performance liquid chromatography PCP, and photocatalyst can reused more than 5 times under the prerequisite that does not reduce catalytic effect.
Description of drawings
Fig. 1 for utilize bismuth silicate for photocatalyst purify waste water in the different starting point concentration PCP processes concentration (wherein catalyst consumption is 250 mg/litre, pH=6.12) over time.
Embodiment
Embodiment 1
In 50 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 2 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree through water-bath.Regularly get 1 ml sample, supernatant is got in spinning, and the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP was greater than 99.0%.
In 50 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 4 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree through water-bath.Regularly get 1 ml sample, get supernatant after the spinning, the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP reached 87.7%.
Embodiment 3
In 50 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 6 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree through water-bath.Regularly get 1 ml sample, get supernatant after the spinning, the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP reached 84.5%.
In 100 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 6 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree through water-bath.Regularly get 1 ml sample, get supernatant after the spinning, the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP reached 91.2%.
Embodiment 5
In 100 milligrams of bismuth silicate powders PCP solution that to be scattered in 200 milliliters of starting point concentrations be 10 mg/litre, under dark condition,, catalyzer is disperseed fully in solution with ultrasonic 10 minutes of mixed solution.Pre-irradiation stirs 30 minutes to reach adsorption equilibrium with mixed solution at the dark condition lower magnetic force earlier, uses 500 watts of xenon lamps (wavelength is 300～800 nanometers) to shine then, and conditioned reaction liquid level and xenon lamp lamp holder spacing are 20 centimetres.Magnetic agitation in the process of photocatalytic degradation is so that reaction solution is even, and the temperature of reaction solution remains on (20 ± 2) degree through water-bath.Regularly get 1 ml sample, get supernatant after the spinning, the sampling back uses HPLC to analyze the concentration of PCP.The result shows that after reaction was carried out 2 hours, the degradation rate of PCP reached 78.1%.
Claims (3)
1. one kind is utilized bismuth silicate for the purify waste water method of middle Woodtreat A (PCP) of photocatalyst, it is characterized in that, comprises the steps:
1) the certain density PCP solution of preparation;
2) in PCP solution, add the bismuth silicate photocatalyst;
3) under the dark condition ultrasonic 10 minutes, the bismuth silicate photocatalyst is dispersed in the PCP solution;
4) mixing solutions that step 3) is obtained stirs to reach the adsorption equilibrium of PCP at the dark condition lower magnetic force;
5) adopt xenon lamp to shine, the temperature of reaction solution keeps constant temperature through water-bath simultaneously;
6) timing sampling, sample thief supernatant after the spinning, the concentration change of analysis PCP;
7) suction filtration reaction solution, the Separation and Recovery photocatalyst.
2. the bismuth silicate that utilizes according to claim 1 is the purify waste water method of middle Woodtreat A (PCP) of photocatalyst, and wherein, in step 1), the starting point concentration of said PCP is 2～10 mg/litre.
3. the bismuth silicate that utilizes according to claim 1 is the purify waste water method of middle Woodtreat A (PCP) of photocatalyst, and it is characterized in that: in the light catalytic purifying step 5) of PCP, described xenon lamp is that wavelength region is 300～800 nanometers, and power is 500 watts xenon lamp.
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| CN103771638B (en) * | 2012-10-26 | 2016-08-10 | 北京师范大学 | A kind of photocatalysis method with ultrasonic atomizatio enhanced sewage treatment effect |
| CN103551098A (en) * | 2013-11-01 | 2014-02-05 | 合肥工业大学 | Method for generating hydroxyl free radical through controlling visible light |
| CN104888401B (en) * | 2015-05-20 | 2017-08-11 | 中国科学院新疆理化技术研究所 | The method of Firebrake ZB alkali metal compound parachlorphenol pollutant dechlorination under photocatalysis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157026A (en) * | 2007-11-08 | 2008-04-09 | 北京师范大学 | A preparation method of bismuth silicate powder photocatalyst |
| CN101638253A (en) * | 2009-09-08 | 2010-02-03 | 北京师范大学 | Method for treating waste water polluted by composite chlorophenol with coordination of visible light-laccase |
| CN101891274A (en) * | 2010-07-27 | 2010-11-24 | 北京师范大学 | Method for coprocessing crystal violet polluted sewage by outdoor natural light-hydrogen peroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157026A (en) * | 2007-11-08 | 2008-04-09 | 北京师范大学 | A preparation method of bismuth silicate powder photocatalyst |
| CN101638253A (en) * | 2009-09-08 | 2010-02-03 | 北京师范大学 | Method for treating waste water polluted by composite chlorophenol with coordination of visible light-laccase |
| CN101891274A (en) * | 2010-07-27 | 2010-11-24 | 北京师范大学 | Method for coprocessing crystal violet polluted sewage by outdoor natural light-hydrogen peroxide |
Non-Patent Citations (2)
| Title |
|---|
| 何莉等.CuO /TiO2 - H2 O2 自然光催化降解印染废水的影响因素.《污染防治技术》.2009,第22卷(第1期),第8-11页. |
| 何莉等.CuO /TiO2- H2 O2 自然光催化降解印染废水的影响因素.《污染防治技术》.2009,第22卷(第1期),第8-11页. * |
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